results of proficiency test styrene october 2016 - iisnl.com · results of proficiency test styrene...

Results of Proficiency Test Styrene October 2016 Organised by: Institute for Interlaboratory Studies (iis) Spijkenisse, the Netherlands Authors: ing. A.S. Noordman - de Neef Correctors: dr. R.G. Visser & ing. R.J. Starink Report: iis16C07 November 2016

Institute for Interlaboratory Studies Spijkenisse, November 2016

page 2 of 42 Styrene: iis16C07

CONTENTS

1 INTRODUCTION ..................................................................................................................................... 3

2 SET UP ..................................................................................................................................................... 3

2.1 ACCREDITATION .................................................................................................................................... 3

2.2 PROTOCOL ............................................................................................................................................. 3

2.3 CONFIDENTIALITY STATEMENT ......................................................................................................... 3

2.4 SAMPLES................................................................................................................................................. 4

2.5 STABILITY OF THE SAMPLES .............................................................................................................. 5

2.6 ANALYSES .............................................................................................................................................. 5

3 RESULTS ................................................................................................................................................. 5

3.1 STATISTICS ............................................................................................................................................. 6

3.2 GRAPHICS ............................................................................................................................................... 6

3.3 Z-SCORES ............................................................................................................................................... 7

4 EVALUATION........................................................................................................................................... 7

4.1 EVALUATION PER TEST ....................................................................................................................... 8

4.2 PERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES ....................................... 11

4.3 COMPARISON OF THE PROFICIENCY TEST OF OCTOBER 2016 WITH PREVIOUS PTS .......... 12

Appendices:

1. Data and statistical results .................................................................................................................... 14

2. Number of participants per country ...................................................................................................... 41

3. Abbreviations and literature .................................................................................................................. 42

Spijkenisse, November 2016 Institute for Interlaboratory Studies

Styrene: iis16C07 page 3 of 42

1 INTRODUCTION

Since 1995, the Institute for Interlaboratory Studies organizes a proficiency test for the

analyses of Styrene. During the annual proficiency testing program 2016/2017, it was

decided to organize again a round robin for the analyses of Styrene in accordance with the

latest applicable version of the product specification ASTM D2827:13. In this interlaboratory

study, 42 laboratories from 20 different countries did register for participation. See

appendix 2 for the number of participants per country. In this report, the results of the 2016

Styrene proficiency test are presented and discussed.

This report is also available as PDF file through the iis website www.iisnl.com.

2 SET UP

The Institute for Interlaboratory Studies (iis) in Spijkenisse, the Netherlands, was the

organiser of this proficiency test (PT). Sample analyses for fit-for-use and homogeneity

testing were subcontracted to an ISO/IEC 17025 accredited laboratory. It was decided to

send one 0.5 litre bottle with Styrene monomer (labelled #16200).

Participants were requested to report the test results using the indicated units and to report

rounded and unrounded test results. The unrounded test results were preferably used for

statistical evaluation.

2.1 ACCREDITATION

The Institute for Interlaboratory Studies in Spijkenisse, the Netherlands, is accredited in

agreement with ISO/IEC 17043:2010 (R007), since January 2000, by the Dutch

Accreditation Council (Raad voor Accreditatie). This proficiency test falls under the

accredited scope. This ensures strict adherence to protocols for sample preparation and

statistical evaluation and 100% confidentially of participant’s data. Feedback from the

participants on the reported data is encouraged and customer’s satisfaction is measured on

regular basis by sending out questionnaires.

2.2 PROTOCOL

The protocol followed in the organisation of this proficiency test was the one as described

for proficiency testing in the report ‘iis Interlaboratory Studies: Protocol for the Organisation,

Statistics and Evaluation’ (iis-protocol, version 3.3) of April 2014. This protocol can be

downloaded from the iis website www.iisnl.com, from the FAQ page.

2.3 CONFIDENTIALITY STATEMENT

All data presented in this report must be regarded as confidential and for use by the

participating companies only. Disclosure of the information in this report is only allowed by

means of the entire report. Use of the contents of this report for third parties is only allowed

by written permission of the Institute for Interlaboratory Studies. Disclosure of the identity of



one or more of the participating companies will be done only after receipt of a written

agreement of the companies involved.

2.4 SAMPLES

The necessary bulk material was obtained from a local Styrene producer. To approximately

36 kg of this batch, the components listed in table 1 were added:

Component Amount

Chloroform 107 mg

Dibenzothiophene 400 mg

Benzene 79 mg

1,2 - Diethylbenzene 1.8 g

n-Propylbenzene 1.8 g

Polystyrene 358 mg Table 1: components added to the bulk materiaal

After homogenisation in a pre-cleaned drum 68 amber glass bottles of 0.5 L (labelled

#16200) were filled. The homogeneity of subsamples of #16200 was checked by

determination of Density at 20°C in accordance with ASTM D4052 and α-Methyl Styrene in

accordance with ASTM D5135 on 8 stratified randomly selected samples.

Density at 20°C in kg/L

α-Methyl Styrene in mg/kg

sample #16200-1 0.90623 202

sample #16200-2 0.90624 199

sample #16200-3 0.90621 197

sample #16200-4 0.90621 199

sample #16200-5 0.90621 198

sample #16200-6 0.90625 199

sample #16200-7 0.90622 201

sample #16200-8 0.90625 200

Table 2: homogeneity test results of subsamples #16200

From the above test results, the repeatabilities were calculated and compared with 0.3

times the corresponding reproducibilities of the reference test methods in agreement with

the procedure of ISO 13528, Annex B2 in the next table:

Density at 20°C in kg/L

α-Methyl Styrene in mg/kg

r (observed) 0.00005 4.5

ref. test method ISO 12185:96 ASTM D5135:14

0.3 x R (ref. test method) 0.00015 10.8 Table 3: evaluation of the repeatabilities of subsamples #16200



The calculated repeatabilities were less than 0.3 times the corresponding reproducibility of the reference test methods. Therefore homogeneity of the subsamples of #16200 was assumed. To each of the participating laboratories, 1 bottle of 0.5 L (labelled #16200) was sent on

September 21, 2016.

2.5 STABILITY OF THE SAMPLES

The stability of Styrene, packed in a brown glass bottle, was checked. The material was

found sufficiently stable for the period of the proficiency test.

2.6 ANALYSES

The participants were asked to determine on sample #16200: Aldehydes as benzaldehyde,

Appearance, Chloride (Organic), Colour Pt/Co, Density at 20°C, Inhibitor as TBC, Peroxide

as H2O2, Polymer, Sulphur, Water (coulometric KF titration), Purity and the Impurities by

GC; Benzene, Toluene, Ethylbenzene, m- & p- Xylenes, Iso-propylbenzene (Cumene),

o-Xylene, n-Propylbenzene, m- & p-Ethyltoluenes, α-Methylstyrene, 1,2-diethylbenzene,

sum α-Methylstyrene and 1,2-diethylbenzene, Phenylacetylene, 3-&4-dimethylstyrenes,

sum Phenylacetylene and 3-&4-dimethylstyrenes, Benzaldehyde and Nonaromatics.

It was explicitely requested to treat the samples as if they were routine samples and to

report the test results using the indicated units on the report form and not to round the

results, but report as much significant figures as possible. Therefore to get comparable test

results a detailed report form, on which the units were prescribed as well as the required

reference test method and a letter of instructions were prepared and made available on the

data entry portal www.kpmd.co.uk/sgs-iis/. The laboratories were also requested to confirm

the sample receipt on the same data entry portal. A SDS was added to the sample.

3 RESULTS

During five weeks after sample dispatch, the test results of the individual laboratories were

gathered via the data entry portal www.kpmd.co.uk/sgs-iis/. The reported test results are

tabulated per determination in appendix 1 of this report. The laboratories are presented by

their code numbers.

Directly after the deadline, a reminder was sent to those laboratories that had not reported

test results at that moment. Shortly after the deadline, the available test results were

screened for suspect data. A test result was called suspect in case the Huber Elimination

Rule (a robust outlier test) found it to be an outlier. The laboratories that produced these

suspect data were asked to check the reported test results (no reanalysis). Additional or

corrected test results are used for data analysis and original test results are placed under

'Remarks' in the test result tables in appendix 1. Test results that came in after the deadline

were not taken into account in this screening for suspect data and thus these participants

were not requested for checks.



3.1 STATISTICS

The protocol followed in the organization of this proficiency test was the one as described

for proficiency testing in the report ‘iis Interlaboratory Studies: Protocol for the Organisation,

Statistics and Evaluation’ of April 2014 (iis-protocol, version 3.3).

For the statistical evaluation the unrounded (when available) figures were used instead of

the rounded test results. Test results reported as ‘<…’ or ‘>…’ were not used in the

statistical evaluation.

First, the normality of the distribution of the various data sets per determination was

checked by means of the Lilliefors-test a variant of the Kolmogorov-Smirnov test and by the

calculation of skewness and kurtosis. Evaluation of the three normality indicators in

combination with the visual evaluation of the graphic Kernel density plot, lead to judgement

of the normality being either ‘unknown’, ‘OK’, ‘suspect’ or ‘not OK’. After removal of outliers,

this check was repeated. Not all data sets proved to have a normal distribution, in which

cases the statistical evaluation of the test results should be used with due care.

According to ISO 5725 the original test results per determination were submitted to Dixon’s,

Grubbs’ and/or Rosner’s outlier tests. Outliers are marked by D(0.01) for the Dixon’s test,

by G(0.01) or DG(0.01) for the Grubbs’ test and by R(0.01) for the Rosner’s test. Stragglers

are marked by D(0.05) for the Dixon’s test, by G(0.05) or DG(0.05) for the Grubbs’ test and

by R(0.05) for the Rosner’s test. Both outliers and stragglers were not included in the

calculations of averages and standard deviations.

For each assigned value the uncertainty was determined in accordance with ISO13528.

Subsequently the calculated uncertainty was evaluated against the respective requirement

based on the target reproducibility in accordance with ISO13528. When the uncertainty

passed the evaluation, no remarks are made in the report. However, when the uncertainty

failed the evaluation it is mentioned in the report and it will have consequences for the

evaluation of the test results.

Finally, the reproducibilities were calculated from the standard deviations by multiplying

them with a factor of 2.8.

3.2 GRAPHICS

In order to visualise the data against the reproducibilities from literature, Gauss plots were

made, using the sorted data for one determination (see appendix 1). On the Y-axis the

reported test results are plotted. The corresponding laboratory numbers are on the X-axis.

The straight horizontal line presents the consensus value (a trimmed mean). The four

striped lines, parallel to the consensus value line, are the +3s, +2s, -2s and -3s target

reproducibility limits of the selected reference test method. Outliers and other data, which

were excluded from the calculations, are represented as a cross. Accepted data are

represented as a triangle.

Furthermore, Kernel Density Graphs were made. This is a method for producing a smooth

density approximation to a set of data that avoids some problems associated with



histograms. Also a normal Gauss curve was projected over the Kernel Density Graph for

reference.

3.3 Z-SCORES

To evaluate the performance of the participating laboratories the z-scores were calculated.

As it was decided to evaluate the performance of the participants in this proficiency test

(PT) against the literature requirements, e.g. ASTM reproducibilities, the z-scores were

calculated using a target standard deviation. This results in an evaluation independent of

the variation of this interlaboratory study. The target standard deviation was calculated from

the literature reproducibility by division with 2.8.

When a laboratory did use a test method with a reproducibility that is significantly different

from the reproducibility of the reference test method used in this report, it is strongly

advised to recalculate the z-score, while using the reproducibility of the actual test method

used, this in order to evaluate whether the reported test result is fit-for-use.

The z-scores were calculated according to: z(target) = (test result - average of PT) / target standard deviation The z(target) scores are listed in the test result tables in appendix 1. Absolute values for z<2 are very common and absolute values for z>3 are very rare. The usual interpretation of z-scores is as follows: | z | < 1 good 1 < | z | < 2 satisfactory 2 < | z | < 3 questionable 3 < | z | unsatisfactory

4 EVALUATION

In this proficiency test some problems were encountered with the dispatch of the samples

to the laboratories in Brazil, United Arab Emirates and India. These laboratories received

the samples late or not at all. One participant reported test results after the final reporting

date and four laboratories did not report any test results at all. Not all participants were able

to report all requested parameters. Finally, 38 laboratories did report 521 numerical test

results. Observed were 14 outlying test results, which is 2.7%. In proficiency studies outlier

percentages of 3 - 7.5% are quite normal.

Not all original data sets proved to have a normal Gaussian distribution. These are referred

to as “not OK” or “suspect”. The statistical evaluation of these data sets should be used

with due care.



4.1 EVALUATION PER TEST

In this section the reported test results are discussed per test. The reference

reproducibilities used for the evaluation of the GC impurities were extrapolated from the

reproducibilities as mentioned in ASTM D5135:14 (table 3 or 4 of the ASTM D5135 test

method) or calculated using the Horwitz equation when no precision data was mentioned in

ASTM D5135:14 or when RD5135<<RHorwitz.

Please note: After closure of the PT a new version of ASTM D5135 was published in

October 2016 and new reproducibilities were published. However, it is decided to use the

reproducibilities of 2014 for the statistical evaluations as this PT took place from September

21 till October 28, 2016. The reproducibilities from ASTM D5135:16 are also mentioned in

the test results tables of appendix 1.

In iis PT reports, ASTM test methods are referred to with a number (e.g. D5808) and an

added designation for the year that the test method was adopted or revised (e.g.

D5808:09a). If applicable, a designation in parentheses is added to designate the year of

reapproval (e.g. D5808:09a (2014)). In the tables of Appendix 1 only the test method

number and year of adoption or revision will be used.

Not all original data sets proved to have a normal Gaussian distribution. These are referred

to as “not OK” or “suspect”. The statistical evaluation of these data sets should be used

with due care, see also paragraph 3.1.

Aldehydes as benzaldehyde: This determination was very problematic. No statistical outliers

were observed. However, the calculated reproducibility is not at all in

agreement with the requirements of ASTM D2119:09. The large variation

was also observed in previous PTs. In iis PT report of 2014 (iis14C07) two

possible root causes are mentioned for this large variation. The first one:

CO2-absorption during the standing period of 1 hour and secondly: the use

of Thymol Blue in stead of the sodium salt of Thymol Blue (and the need of

caustic to dissolve the Thymol blue). None of the participants reported a

value lower than the Benzaldehyde content by GC.

Appearance: Allthough not mentioned in ASTM D2827:13, the specification of Styrene; it

is advised to use test method ASTM E2680:09(2015)e1 for the appearance

determination. All participants agreed about the appearance of sample

#16200 to be ‘clear and bright’ or ‘pass’. Participants who used ASTM

E2680 should report the appearance as ‘pass’ or as ‘fail’ dependent on the

appearance of the product.

Chloride, Organic: This determination was not problematic. One statistical outlier was

observed. The calculated reproducibility after rejection of the statistical

outlier is in good agreement with the requirements of ASTM D5808:09a

(2014). The average recovery of Inorganic Chloride (theoretical increment

of 2.7 mg Cl/kg) may be acceptable: “less than 79%” (the actual blank

Chloride content is unknown).



Colour Pt/Co: This determination was not problematic. No statistical outliers were

observed. The calculated reproducibility is in good agreement with the

requirements of ASTM D5386:10 and with ASTM D1209:05(2011).

Density at 20°C: This determination was not problematic. One statistical outlier was

observed. The calculated reproducibility after rejection of the statistical

outlier is in good agreement with the requirements of ISO 12185:96.

Inhibitor as TBC: This determination was not problematic. Two statisticals outliers were

observed. However, the calculated reproducibility after rejection of the

statistical outliers is in full agreement with the requirements of ASTM

D4590:13.

Peroxides as H2O2: This determination was problematic. One statistical outlier was observed.

The calculated reproducibility after rejection of the statistical outlier is not in

agreement with the requirements of ASTM D2340:13.

Polymers: This determination was problematic. No statistical outliers were observed. However, the calculated reproducibility is not in agreement with the requirements of ASTM D2121-A:16.

The average recovery of Polymer (theoretical increment of 10.1 mg Polymer/kg) may be good: “less than 82%” (the actual blank Polymer content is unknown).

Sulphur: This determination was not problematic. One statistical outlier was observed. The calculated reproducibility after rejection of the statistical outlier is in good agreement with the requirements of ASTM D5453:16e1.

The average recovery of Sulphur (theoretical increment of 2.0 mg Sulphur /kg) may be very good: “less than 97%” (the actual blank Sulphur content is unknown).

Water, coulometric KF titration: This determination was not problematic. No statistical outliers

were observed. The calculated reproducibility is in good agreement with the

requirement of ASTM E1064:16.

Purity by GC: This determination was not problematic. No statistical outliers were

observed. The calculated reproducibility is in full agreement with the

requirements of ASTM D5135:14.

Benzene: This determination was problematic. One statistical outlier was observed. The calculated reproducibility after rejection of the statistical outlier is not in agreement with the requirements of ASTM D6229:06(2010).

The average recovery of Benzene (theoretical increment of 2.2 mg Benzene/kg) may be very good: “less than 98%” (the actual blank Benzene content is unknown). Ten participants reported a Benzene value “<10 mg/kg”. It should be noted that the Styrene specification D2827:13 mentions a Benzene content of 1 mg/kg maximum and thus reporting ‘<10 mg/kg’ is not in accordance with the D2827 specification.



Toluene: About 77% of the reporting participants reported a Toluene value “less than” and other reported test values were below or near the application range. Therefore no significant conclusions were drawn. One false positive test result was reported.

Ethylbenzene: This determination was not problematic. No statistical outliers were

observed. The calculated reproducibility is in good agreement with the


m- & p-Xylenes: About 68% of the reporting participants reported a value “less than” and other reported test values were below or near the application range. Therefore no significant conclusions were drawn. No false positive test results were reported.

iso-Propylbenzene (Cumene): About 69% of the reporting participants reported a value “less than” and other reported test values were below or near the application range. Therefore no significant conclusions were drawn. No false positive test results were reported.

o-Xylene: About 74% of the reporting participants reported a value “less than” and other reported test values were below or near the application range. Therefore no significant conclusions were drawn. Two false positive test results were reported.

n-Propylbenzene: This determination was not problematic. Two statisticals outliers were observed. However, the calculated reproducibility after rejection of the statistical outliers is in agreement with the requirements of ASTM D5135:14. Two false negative test results were reported.

The average recovery of n-Propylbenzene (theoretical increment of 50.3 mg n-Propylbenzene /kg) may be acceptable: “less than 125%” (the actual blank n-Propylbenzene content is unknown).

m-& p-Ethyltoluenes: This determination was not problematic. One statistical outlier was observed and one false negative test result was reported. The calculated reproducibility after rejection of the statistical outlier is in agreement with the requirements of ASTM D5135:14.

α-Methylstyrene: This determination was problematic. No statistical outliers were observed.

However, the calculated reproducibility is not in agreement with the


1,2-Diethylbenzene: Only four laboratories reported a numerical test result for this component. Therefore no z-scores were calculated. Two false negative test results were reported.

Surprisingly, the average recovery based on 4 reported test results of 1,2-Diethylbenzene (theoretical increment of 50.5 mg 1,2-Diethylbenzene /kg) may be very good: “less than 95%” (the actual blank 1,2-Diethylbenzene content is unknown).



Sum α-Methylstyrene & 1,2-Diethylbenzene: Only eight laboratories reported a numerical test

result for the sum of the two components. However, this determination may

be not problematic. No statistical outliers were observed. The calculated

reproducibility is in agreement with the estimated requirements using the

Horwitz equation for two components.

Phenylacetylene: About 64% of the reporting participants reported a value “less than” and other reported test values were below or near the application range. Therefore no significant conclusions were drawn. No false positive test results were reported.

3-&4-Methylstyrenes: Three laboratories reported a numeric test result and four reported a test value as “lower than”. Therefore, no significant conclusions could be drawn. One false positive test result was reported.

Sum Phenylacetylene & 3- & 4 -Methylstyrenes: Only six laboratories reported a numerical test result for the sum of the three components. However, this determination may not problematic. One statistical outlier was observed and one false negative test result was reported. The calculated reproducibility after rejection of the statistical outlier is in good agreement with the estimated requirements using the Horwitz equation for three components.

Benzaldehyde: This determination may be problematic. No statistical outliers were

observed and one false negative test result was reported. However, the

calculated reproducibility is not in agreement with the estimated

requirements using the Horwitz equation, but it is in agreement with the


Nonaromatics: This determination may be very problematic. No statistical outliers were

observed and one false negative test result was reported. The calculated

reproducibility is not in agreement with the estimated requirements using

the Horwitz equation for nine components. The number of nonaromatic

impurities is not known but expected to be many; hence the choice for nine

components. The calculated reproducibility is also not in agreement with

the requirements of ASTM D5135:16.

4.2 PERFORMANCE EVALUATION FOR THE GROUP OF LABORATORIES

A comparison has been made between the reproducibility as declared by the relevant

reference test method and the reproducibility as found for the group of participating

laboratories. The target reproducibilities derived from reference test methods (in casu

ASTM reference test methods) and the calculated reproducibilities of sample #16200 are

compared in the next table.



Parameter unit n average 2.8 *sd R (lit)

Aldehydes as benzaldehyde mg/kg 29 109.5 65.5 43.8

Appearance 34 Pass n.a. n.a.

Chloride, Organic mg/kg 13 2.3 1.1 1.3

Colour Pt/Co 38 9.0 4.2 6.0

Density at 20°C kg/L 33 0.9063 0.0002 0.0005

Inhibitor as TBC mg/kg 33 9.2 3.2 3.1

Peroxides as H2O2 mg/kg 26 18.4 21.1 13.0

Polymers mg/kg 34 8.2 9.4 7.9

Sulphur mg/kg 25 1.9 0.7 1.0

Water, coulometric KF titration mg/kg 35 161 25 45

Purity by GC %M/M 34 99.94 0.03 0.03

Benzene mg/kg 19 2.2 1.8 1.2

Toluene mg/kg 22 <10 n.a. n.a.

Ethylbenzene mg/kg 33 56.6 12.2 16.2

m- & p-Xylenes mg/kg 28 <10 n.a. n.a.

iso-Propylbenzene (Cumene) mg/kg 29 <10 n.a. n.a.

o-Xylene mg/kg 23 <10 n.a. n.a.

n-Propylbenzene mg/kg 22 62.8 11.3 15.7

m- & p-Ethyltoluenes mg/kg 10 9.0 2.5 3.2

α-Methylstyrene mg/kg 28 229 69 38

1,2-Diethylbenzene mg/kg 4 47.9 53.3 (12.0)

sum α-Methylstyrene & 1,2-diethylbenzene mg/kg 8 249 74 69

Phenylacetylene mg/kg 22 <10 n.a. n.a.

3- & 4-Methylstyrenes mg/kg 6 <10 n.a. n.a.

sum Phenylacetylene & 3- & 4-Methylstyrenes mg/kg 5 10.6 5.3 5.8

Benzaldehyde mg/kg 16 64.0 23.8 15.3

Nonaromatics mg/kg 15 61.0 83.3 44.1 Table 4: comparison of the observed and target reproducibilities of sample #16200 Figure under R(lit) between brackets is based on very little test results

Without further statistical calculations it can be concluded that for only several components

there is a good compliance of the group of participating laboratories with the relevant reference

test methods. The components that are problematic have been discussed in paragraph 4.1.

4.3 COMPARISON OF THE PROFICIENCY TEST OF OCTOBER 2016 WITH PREVIOUS PTS

October

2016 October

2015 September

2014 September

2013 September

2012

Number of reporting labs 38 37 36 34 38

Number of test results reported 521 447 510 474 552

Number of statistical outliers 14 20 33 29 30

Percentage outliers 2.7% 4.5% 6.5% 6.1% 5.4% Table 5: comparison with previous proficiency tests

In proficiency tests, outlier percentages of 3% - 7.5% are quite normal.



The performance of the determinations of the proficiency tests was compared against the

requirements of the respective reference test methods. The conclusions are given in the

following table:

Determination October

2016 October

2015 September

2014 September

2013 September

2012

Aldehydes as benzaldehyde - -- -- -- --

Chloride, Organic + n.e. + +/- ++

Colour Pt/Co + ++ ++ ++ +

Density at 20°C ++ ++ ++ ++ ++

Inhibitor as TBC +/- + -- -- +

Peroxides as H2O2 - - -- -- --

Polymers - ++ -- -- --

Sulphur + n.e. + ++ +

Water, coulometric KF titration + + ++ -- --

Purity by GC +/- + (--) ++ +/-

Benzene - n.e. -- -- --

Toluene n.e. n.e. -- n.e. n.e.

Ethylbenzene + ++ ++ ++ +/-

m- & p-Xylenes n.e. ++ ++ -- --

iso-Propylbenzene (Cumene) n.e. - -- n.e. +

o-Xylene n.e. ++ -- ++ ++

n-Propylbenzene + (--) -- + n.e.

m- & p-Ethyltoluenes + (-) ++ n.e. n.e.

α-Methylstyrene -- ++ -- -- -

1,2-Diethylbenzene (--) n.e. (--) n.e. n.e.

sum α-Methylstyrene & 1,2-diethylbenzene +/- ++ n.e. n.e. n.e.

Phenylacetylene n.e. n.e. -- -- (--)

3- & 4-Methylstyrenes n.e. n.e. n.e. -- n.e.

sum Phenylacetylene & 3- & 4-Methylstyrenes + n.e. n.e. n.e. n.e.

Benzaldehyde - - -- -- --

Nonaromatics -- n.e. -- n.e. n.e. Table 6: comparison of overall performance against the requirement of the reference test method per parameter

Between brackets is near or below the detection limit of the test method

The performance of the determinations against the requirements of the respective reference test methods is listed in the above table. The following performance categories were used:

++ : group performed much better than the reference test method

+ : group performed better than the reference test method

+/-: group performance equals the reference test method

- : group performed worse than the reference test method

-- : group performed much worse than the reference test method

n.e.: not evaluated



APPENDIX 1 Determination of Aldehydes as benzaldehyde on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D2119 105 -0.29 169 D2119 120 0.67 171 D2119 98 -0.74 173 D2119 94 -0.99 174 D2119 93 -1.06 273 ----- ----- 311 D2119 110 0.03 323 D2119 120 0.67 333 D2119 70 -2.53 343 D2119 116 0.41 347 D2119 112 0.16 396 ----- ----- 446 D2119 80 -1.89 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D2119 134 1.57 858 D2119 130.0 1.31 860 D2119 128 1.18 862 D2119 130 1.31 863 D2119 125 0.99 868 D2119 130 1.31 869 D2119 115 0.35 902 D2119 110 0.03 913 ----- -----

1067 D2119 92 -1.12 1107 D2119 121 0.73 1117 D7704 72 -2.40 1201 ----- ----- 1252 ----- ----- 1264 ----- ----- 1319 140 1.95 1429 109.4 -0.01 1509 D2119 73 -2.33 1515 D2119 71.34 -2.44 1767 D2119 156.8 3.02 1823 D2119 139.3 1.90 1866 ----- ----- 1880 D7704 81.0 -1.82 6013 ----- ----- 7014 ----- ----- 9008 In house ----- W ----- first reported: 57.7

normality OK n 29 outliers 0 mean (n) 109.51 st.dev. (n) 23.406 R(calc.) 65.54 R(D2119:09) 43.80

0

20

40

60

80

100

120

140

160

180

333

1515

1117

1509

446

1880

1067

174

173

171

150

1429

311

902

347

869

343

169

323

1107

863

860

862

858

868

857

1823

1319

1767 0

0.002

0.004

0.006

0.008

0.01

0.012

0.014

0.016

0.018

0 50 100 150 200

Kernel Density



Determination of Appearance on sample #16200;

lab method value mark z(targ) remarks 150 E2680 Pass ----- 169 D4176 BC&FSM ----- 171 E2680 Pass ----- 173 D4176 Pass ----- 174 E2680 CFSM ----- 273 E2680 Pass ----- 311 E2680 pass ----- 323 Visual clear & bright ----- 333 ----- ----- 343 E2680 Pass ----- 347 E2680 PASS ----- 396 E2680 Pass ----- 446 E2680 Pass ----- 551 ----- ----- 557 ----- ----- 613 E2680 PASS ----- 857 E2680 Pass ----- 858 ----- ----- 860 Visual Bright & Clear ----- 862 E2680 Pass ----- 863 E2680 Pass ----- 868 E2680 pass ----- 869 Visual Clear and bright ----- 902 E2680 PASS ----- 913 E2680 CFSM -----

1067 E2680 Pass ----- 1107 E2680 pass ----- 1117 D4176 pass ----- 1201 Visual Clear and free ----- 1252 Visual PASS ----- 1264 ----- ----- 1319 Clear & Bright ----- 1429 E2680 Pass ----- 1509 E2680 Clear & Free from suspended matter ----- 1515 E2680 PASS ----- 1767 ----- ----- 1823 Visual Clear/FFSM/No free water ----- 1866 ----- ----- 1880 Visual Pass ----- 6013 ----- ----- 7014 Visual Clear ----- 9008 Visual Clear liquid -----

n 34 outliers 0 mean (n) Pass



Determination of Chloride, Organic on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D7359 2.3 -0.02 169 ----- ----- 171 D5808 1 D(0.05) -2.82 173 ----- ----- 174 ----- ----- 273 ----- ----- 311 D5808 2 -0.66 323 D5808 2 -0.66 333 ----- ----- 343 ----- ----- 347 D5808 2.06 -0.53 396 ----- ----- 446 ----- ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 ----- ----- 858 ----- ----- 860 ----- ----- 862 ----- ----- 863 ----- ----- 868 D5808 1.4 -1.96 869 ----- ----- 902 ----- ----- 913 ----- -----

1067 UOP779 2.6 0.63 1107 ----- ----- 1117 ----- ----- 1201 D5808 2.2 -0.23 1252 ----- ----- 1264 ----- ----- 1319 3 1.49 1429 D7359 2.4 0.20 1509 D5808 2.321 0.03 1515 ----- ----- 1767 D5808 2.42 0.24 1823 ----- ----- 1866 ----- ----- 1880 D7359 2.7 0.84 6013 ----- ----- 7014 ----- ----- 9008 D5808 2.6 0.63

normality suspect n 13 outliers 1 spike mean (n) 2.31 2.7 (recovery: <79%) st.dev. (n) 0.399 R(calc.) 1.12 R(D5808:09a) 1.30

0

0.5

1

1.5

2

2.5

3

3.5

4

171

868

323

311

347

1201

150

1509

1429

1767

1067

9008

1880

1319 0

0.2

0.4

0.6

0.8

1

1.2

0 1 2 3 4

Kernel Density



Determination of Colour Pt/Co on sample #16200;

lab method value mark z(targ) remarks 150 D5386 9 -0.02 169 D5386 10.2 0.54 171 D1209 10 0.45 173 D5386 10 0.45 174 D5386 8.5 -0.25 273 D1209 7.4 -0.76 311 D5386 9 -0.02 323 D5386 8 -0.48 333 D5386 9 -0.02 343 D5386 10 0.45 347 D5386 9 -0.02 396 D5386 9 -0.02 446 D5386 7 -0.95 551 ----- ----- 557 ----- ----- 613 D1209 5 -1.88 857 D5386 10 0.45 858 D5386 9 -0.02 860 D5386 10.3 0.59 862 D5386 10 0.45 863 D1209 9 -0.02 868 D5386 10.8 0.82 869 D1209 8 -0.48 902 D5386 9 -0.02 913 D5386 6 -1.42

1067 D5386 8.7 -0.16 1107 D5386 8.3 -0.34 1117 D1209 10 0.45 1201 D5386 7 -0.95 1252 D1209 9.70 0.31 1264 ----- ----- 1319 9 -0.02 1429 D5386 12 1.38 1509 D1209 10 0.45 1515 D1209 8 -0.48 1767 D5386 11.0 0.92 1823 D5386 10.7 0.78 1866 ----- ----- 1880 D5386 11.0 0.92 6013 D5386 7 -0.95 7014 D1209 7 -0.95 9008 D5386 10.8 0.82

normality OK n 38 outliers 0 mean (n) 9.04 st.dev. (n) 1.510 R(calc.) 4.23 R(D5386:10) 6.00 compare R(D1209:05(2011)) = 7

0

2

4

6

8

10

12

14

16

18

613

913

446

1201

6013

7014

273

323

869

1515

1107

174

1067

396

150

311

333

347

858

863

902

1319

1252

857

173

343

171

862

1117

1509

169

860

1823

868

9008

1767

1880

1429 0

0.05

0.1

0.15

0.2

0.25

0.3

0 5 10 15

Kernel Density



Determination of Density at 20°C on sample #16200; results in kg/L

lab method value mark z(targ) remarks 150 D4052 0.9064 0.56 169 D4052 0.9063 0.00 171 D4052 0.8610 R(0.01) -253.68 173 D4052 0.9064 0.56 174 D4052 0.9063 0.00 273 ----- ----- 311 ISO12185 0.90628 -0.11 323 D4052 0.9063 0.00 333 ISO12185 0.9062 -0.56 343 D4052 0.90632 0.11 347 D4052 0.90624 -0.33 396 D4052 0.9063 0.00 446 D4052 0.9066 1.68 551 ----- ----- 557 ----- ----- 613 D4052 0.9064 0.56 857 D4052 0.90626 -0.22 858 D4052 0.90626 -0.22 860 D4052 0.90627 -0.17 862 D4052 0.90628 -0.11 863 D4052 0.90631 0.06 868 D4052 0.90627 -0.17 869 D4052 0.90629 -0.05 902 D4052 0.9064 0.56 913 D4052 0.9063 0.00

1067 D4052 0.9063 0.00 1107 D4052 0.90626 -0.22 1117 D4052 0.9063 0.00 1201 D4052 0.9061 -1.12 1252 D4052 0.9064 0.56 1264 ----- ----- 1319 0.9062 -0.56 1429 D4052 0.9064 0.56 1509 D4052 0.90630 0.00 1515 ----- ----- 1767 D4052 0.9062 -0.56 1823 D4052 0.9063 0.00 1866 ----- ----- 1880 D4052 0.9062 -0.56 6013 ----- ----- 7014 D4052 0.90625 -0.28 9008 ----- -----

normality not OK n 33 outliers 1 mean (n) 0.90630 st.dev. (n) 0.000087 R(calc.) 0.00024 R(ISO12185:96) 0.00050

0.9055

0.9057

0.9059

0.9061

0.9063

0.9065

0.9067

0.9069

0.9071

171

1201

333

1319

1767

1880

347

7014

858

857

1107

860

868

862

311

869

174

396

169

323

913

1067

1117

1509

1823

863

343

173

613

150

902

1252

1429

446 0

500

1000

1500

2000

2500

3000

3500

4000

4500

0.9055 0.906 0.9065 0.907

Kernel Density



Determination of Inhibitor as TBC on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D4590 7.6 -1.44 169 D4590 9.2 0.02 171 D4590 7 -1.98 173 ----- ----- 174 D4590 49.95 R(0.01) 37.15 273 D4590 11.32 C 1.95 first reported: 13.7 311 D4590 10 0.75 323 D4590 8 -1.07 333 D4590 10 0.75 343 ----- ----- 347 D4590 9.6 0.38 396 D4590 10.7 1.39 446 D4590 11 1.66 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D4590 8.4 -0.71 858 D4590 9.1 -0.07 860 D4590 8.6 -0.53 862 D4590 8.4 -0.71 863 D4590 8.3 -0.80 868 D4590 8.5 -0.62 869 D4590 8.3 -0.80 902 D4590 9.8 0.57 913 D4590 5.64 R(0.05) -3.22

1067 D4590 9.9 0.66 1107 D4590 9.2 0.02 1117 D4590 10.5 1.20 1201 D4590 9.9 0.66 1252 D4590 9.56 0.35 1264 ----- ----- 1319 8.9 -0.25 1429 D4590 6.9 -2.08 1509 D4590 8.918 -0.24 1515 D4590 9.393 0.20 1767 D4590 8.60 -0.53 1823 D4590 8.5 -0.62 1866 ----- ----- 1880 D4590 7.9 -1.16 6013 D4590 9.3 0.11 7014 D4590 11.59 2.20 9008 In house 10 0.75


3

4

5

6

7

8

9

10

11

12

13

913

1429

171

150

1880

323

869

863

862

857

868

1823

860

1767

1319

1509

858

169

1107

6013

1515

1252

347

902

1067

1201

311

333

9008

1117

396

446

273

7014

174 0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0 5 10 15

Kernel Density



Determination of Peroxides as H2O2 on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D2340 11 -1.59 169 D2340 12 -1.37 171 D2340 9 -2.02 173 D2340 14.8 -0.77 174 D2340 92.19 R(0.01) 15.90 273 ----- ----- 311 D2340 13 -1.16 323 D2340 24 1.21 333 ----- ----- 343 ----- ----- 347 D2340 8 -2.23 396 ----- ----- 446 D2340 8 -2.23 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D2340 20 0.35 858 ----- ----- 860 ----- ----- 862 D2340 17.8 -0.12 863 D2340 19.4 0.22 868 D2340 29.0 2.29 869 D2340 20 0.35 902 ----- ----- 913 D2340 35.15 3.61

1067 D2340 9.4 -1.93 1107 ----- ----- 1117 D2340 18.7 0.07 1201 D2340 9.2 -1.98 1252 D2340 25.50 1.53 1264 ----- ----- 1319 16 -0.51 1429 D2340 21.6 0.69 1509 D2340 34.3 3.43 1515 ----- ----- 1767 D2340 23.1 1.02 1823 D2340 15.4 -0.64 1866 ----- ----- 1880 D2340 20.4 0.44 6013 D2340 21 0.57 7014 ----- ----- 9008 D2340 22 C 0.78 first reported: 40


0

5

10

15

20

25

30

35

40

45

50

347

446

171

1201

1067

150

169

311

173

1823

1319

862

1117

863

869

857

1880

6013

1429

9008

1767

323

1252

868

1509

913

174 0

0.01

0.02

0.03

0.04

0.05

0.06

-5 15 35

Kernel Density



Determination of Polymers on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D2121-A 5.6 -0.94 169 D2121-A 8 -0.09 171 D2121-A 4 -1.51 173 D2121-A 3.7 -1.61 174 D2121-A 5.096 -1.12 273 D2121-A 1.0 -2.57 311 D2121-A 8 -0.09 323 D2121-A 14 2.05 333 D2121-A 1.5 -2.40 343 ----- ----- 347 D2121-A 8 -0.09 396 ----- ----- 446 D2121-A 1 -2.57 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D2121-A 7.4 -0.30 858 D2121-A 8.8 0.20 860 D2121-A 8.7 0.16 862 D2121-A 8.6 0.13 863 D2121-A 8.5 0.09 868 D2121-A 10.2 0.70 869 D2121-A 9.0 0.27 902 ----- ----- 913 D2121-A 13.24 1.78

1067 D2121-A 9.3 0.38 1107 D2121-A 11.45 1.14 1117 D2121-A 11.6 1.19 1201 D2121-A 9.4 0.41 1252 D2121-A 9.56 0.47 1264 ----- ----- 1319 7.4 -0.30 1429 D2121-A 7.9 -0.12 1509 D2121-A 9.43 0.42 1515 D2121-A 11.579 1.19 1767 D2121-A 13.9 2.01 1823 D2121-A 12.4 1.48 1866 ----- ----- 1880 D2121-A 7.2 -0.37 6013 D2121-A 10 0.62 7014 D2121-A 8.82 0.20 9008 D2121-A 6.0 -0.80

normality OK n 34 outliers 0 spike mean (n) 8.24 10.1 (recovery: <82%) st.dev. (n) 3.339 R(calc.) 9.35 R(D2121-A:16) 7.88

0

2

4

6

8

10

12

14

16

18

446

273

333

173

171

174

150

9008

1880

857

1319

1429

169

347

311

863

862

860

858

7014

869

1067

1201

1509

1252

6013

868

1107

1515

1117

1823

913

1767

323 0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

-5 0 5 10 15 20

Kernel Density



Determination of Sulphur on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5453 2.04 0.29 169 ----- ----- 171 D5453 2.0 0.17 173 ----- ----- 174 D5453 0.274 R(0.01) -4.90 273 D5453 2.7 2.23 311 D5453 2.0 0.17 323 D5453 2 0.17 333 ----- ----- 343 D5453 2.07 0.38 347 D5453 1.77 -0.51 396 ----- ----- 446 ----- ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D3120 2 0.17 858 D5453 1.7 -0.71 860 D3120 1.8 -0.42 862 D5453 1.7 -0.71 863 D5453 2.00 0.17 868 D5453 1.8 -0.42 869 ----- ----- 902 ----- ----- 913 D5453 1.50 -1.30

1067 D5453 2.0 0.17 1107 ----- ----- 1117 D5453 2.2 0.76 1201 D5453 1.8 -0.42 1252 D5453 <1 <-2.76 possibly a false negative test result? 1264 ----- ----- 1319 1.7 -0.71 1429 D5453 1.9 -0.12 1509 D5453 1.91 -0.09 1515 ----- ----- 1767 D5453 1.72 -0.65 1823 D5453 2.01 0.20 1866 ----- ----- 1880 D5453 2.3 1.05 6013 ----- ----- 7014 D5453 2.23 0.85 9008 D5453 1.7 -0.71

normality not OK n 25 outliers 1 spike mean (n) 1.942 2.0 (recovery: <97%) st.dev. (n) 0.2479 R(calc.) 0.694 R(D5453:16e1) 0.954

0

0.5

1

1.5

2

2.5

3

3.5

174

913

858

862

1319

9008

1767

347

860

868

1201

1429

1509

863

171

857

311

323

1067

1823

150

343

1117

7014

1880

273 0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8

-1 0 1 2 3 4

Kernel Density



Determination of Water, coulometric KF titration on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D6304 160 -0.06 169 E1064 158 -0.19 171 E1064 151.8 -0.58 173 D6304 159 -0.13 174 E1064 177.9 1.06 273 ----- ----- 311 E1064 150 -0.69 323 E1064 165 0.25 333 ----- ----- 343 E1064 160.4 -0.04 347 E1064 168 0.44 396 E1064 163 0.12 446 E1064 159 -0.13 551 ----- ----- 557 ----- ----- 613 E203 156.6 -0.28 857 E1064 168 0.44 858 E1064 159 -0.13 860 E1064 160 -0.06 862 E1064 162 0.06 863 E1064 164 0.19 868 E1064 161 0.00 869 E1064 155 -0.38 902 E1064 168 0.44 913 E1064 170 0.56

1067 E1064 153 -0.50 1107 E1064 161 0.00 1117 E1064 168 0.44 1201 E1064 160 -0.06 1252 E1064 188 1.69 1264 ----- ----- 1319 155 -0.38 1429 E1064 156 -0.32 1509 E1064 163 0.12 1515 E1064 154 -0.44 1767 E1064 181.7 1.30 1823 E1064 151.8 -0.58 1866 ----- ----- 1880 D6304 146 -0.94 6013 ----- ----- 7014 E1064 147.98 -0.82 9008 E1064 154.9 -0.38

normality not OK n 35 outliers 0 mean (n) 161.03 st.dev. (n) 8.960 R(calc.) 25.09 R(E1064:16) 44.61

80

100

120

140

160

180

200

220

1880

7014

311

171

1823

1067

1515

9008

869

1319

1429

613

169

858

446

173

150

860

1201

343

868

1107

862

396

1509

863

323

347

857

902

1117

913

174

1767

1252 0

0.01

0.02

0.03

0.04

0.05

0.06

125 145 165 185 205

Kernel Density



Determination of Purity by GC on sample #16200; results in %M/M

lab method value mark z(targ) remarks 150 D5135 99.92 -1.79 169 D5135 99.9324 -0.74 171 D5135 99.935 -0.52 173 D5135 99.929 -1.03 174 D5135 99.96 1.60 273 D5135 99.94 C -0.10 first reported: 99.87 311 D5135 99.95 0.75 323 D5135 99.95 0.75 333 D5135 99.93 -0.95 343 D5135 99.96 1.60 347 D5135 99.936 -0.44 396 ----- ----- 446 D5135 99.96 1.60 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 99.933 -0.69 858 D5135 99.945 0.33 860 D5135 99.945 0.33 862 D5135 99.946 0.41 863 D5135 99.938 -0.27 868 D5135 99.949 0.67 869 D5135 99.956 1.26 902 D5135 99.95 0.75 913 D5135 99.952 0.92

1067 D5135 99.95 0.75 1107 D5135 99.95 0.75 1117 D5135 99.938 -0.27 1201 D5135 99.91 -2.64 1252 D5135 99.934 -0.61 1264 ----- ----- 1319 99.94 -0.10 1429 ----- ----- 1509 D5135 99.917 -2.05 1515 D7504 99.9554 1.21 1767 D5135 99.934 -0.61 1823 D5135 99.938 -0.27 1866 ----- ----- 1880 D5135 99.940 -0.10 6013 ----- ----- 7014 D5135 99.937 -0.35 9008 D5135 99.94 -0.10

normality OK n 34 outliers 0 mean (n) 99.9411 st.dev. (n) 0.01199 R(calc.) 0.0336 R(D5135:14) 0.0330 compare R(D1535:16) = 0.0295

99.9

99.91

99.92

99.93

99.94

99.95

99.96

99.97

99.98

99.99

1201

1509

150

173

333

169

857

1252

1767

171

347

7014

863

1117

1823

273

1319

1880

9008

858

860

862

868

323

311

902

1067

1107

913

1515

869

343

446

174 0

5

10

15

20

25

30

35

99.88 99.9 99.92 99.94 99.96 99.98 100

Kernel Density



Determination of Benzene on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 3 C 1.93 first reported: 4 169 D5135 2 -0.34 171 ----- ----- 173 D7504 2 -0.34 174 D5135 <10 ----- 273 ----- ----- 311 D5135 2 -0.34 323 D6229 1 -2.60 333 ----- ----- 343 2.25 0.23 347 INH-CM3015 2.1 -0.11 396 ----- ----- 446 D5135 <10 ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 <10 ----- 858 D5135 <10 ----- 860 D5135 <10 ----- 862 D5135 <10 C ----- first reported: 5 863 D5135 <10 C ----- first reported: 4 868 D5135 <10 ----- 869 D5135 <10 ----- 902 INH-123 <10 ----- 913 D5135 6 R(0.01) 8.73

1067 0.6 -3.51 1107 D5135 2 -0.34 1117 In house 2.27 0.28 1201 In house 2.3 0.34 1252 D5135 2.70 1.25 1264 ----- ----- 1319 1.8 -0.79 1429 ----- ----- 1509 In house 2.47 0.73 1515 INH-2922 2 C -0.34 first reported: 5.96 1767 ----- ----- 1823 D6229 2.32 0.39 1866 ----- ----- 1880 D4534 2.1 -0.11 6013 ----- ----- 7014 D5135 3.6 3.29 9008 D6229 2.3 0.34

normality not OK n 19 outliers 1 spike mean (n) 2.15 2.2 (recovery: <98%) st.dev. (n) 0.637 R(calc.) 1.78 R(D6229:06) 1.23 compare R(Horwitz) = 0.86 and R(D1535:16) = 0.92

0

1

2

3

4

5

6

7

1067

323

1319

173

169

311

1107

1515

347

1880

343

1117

1201

9008

1823

1509

1252

150

7014

913 0

0.2

0.4

0.6

0.8

1

1.2

0 2 4 6 8

Kernel Density



Determination of Toluene on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 15 D(0.05) ----- possibly a false positive test result? 169 ----- ----- 171 D5135 <1 ----- 173 D7504 <1 ----- 174 D5135 <10 ----- 273 ----- ----- 311 D5135 <10 ----- 323 D5135 <1 ----- 333 ----- ----- 343 ----- ----- 347 ----- ----- 396 ----- ----- 446 D5135 <10 ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 <10 ----- 858 D5135 <10 ----- 860 D5135 <10 ----- 862 D5135 <1 ----- 863 D5135 <10 ----- 868 D5135 <10 ----- 869 ----- ----- 902 ----- ----- 913 D5135 nd -----

1067 ----- ----- 1107 D5135 <10 ----- 1117 D5135 2 ----- 1201 D5135 5 ----- 1252 D5135 3.50 ----- 1264 ----- ----- 1319 2.2 ----- 1429 ----- ----- 1509 D5135 <5 ----- 1515 D7504 <5 ----- 1767 ----- ----- 1823 D5135 <10 ----- 1866 ----- ----- 1880 ----- ----- 6013 ----- ----- 7014 D5135 0.9 ----- 9008 <1 -----

normality n.a. n 22 outliers 1 mean (n) <10 st.dev. (n) n.a. R(calc.) n.a. R(lit) n.a.



Determination of Ethylbenzene on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 59 0.42 169 D5135 55 -0.27 171 D5135 50 -1.14 173 D5135 56 -0.10 174 D5135 49.03 -1.31 273 ----- ----- 311 D5135 60 0.60 323 D5135 61 0.77 333 D5135 63 1.11 343 D5135 55 -0.27 347 D5135 56 -0.10 396 ----- ----- 446 D5135 49 -1.31 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 58 0.25 858 D5135 60 0.60 860 D5135 56 -0.10 862 D5135 56 -0.10 863 D5135 56 -0.10 868 D5135 53 -0.62 869 D5135 62 0.94 902 D5135 65 1.46 913 D5135 56 -0.10

1067 D5135 60 0.60 1107 D5135 58 0.25 1117 D5135 58 0.25 1201 D5135 52 -0.79 1252 D5135 61.5 0.86 1264 ----- ----- 1319 51.8 -0.83 1429 ----- ----- 1509 D5135 62 0.94 1515 D7504 46 -1.83 1767 D5135 58 C 0.25 first reported: 0.0058 mg/kg 1823 D5135 58.6 0.35 1866 ----- ----- 1880 D5135 55.8 -0.13 6013 ----- ----- 7014 D5135 56.1 -0.08 9008 D5135 53.8 -0.48

normality OK n 33 outliers 0 mean (n) 56.56 st.dev. (n) 4.365 R(calc.) 12.22 R(D5135:14) 16.16 compare R(Horwitz) = 13.80 and R(D1535:16) = 10.81

30

35

40

45

50

55

60

65

70

75

80

1515

446

174

171

1319

1201

868

9008

169

343

1880

173

860

863

347

862

913

7014

857

1107

1117

1767

1823

150

311

858

1067

323

1252

869

1509

333

902 0

0.01

0.02

0.03

0.04

0.05

0.06

0.07

0.08

0.09

0.1

30 40 50 60 70 80

Kernel Density



Determination of m- & p-Xylenes on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 5 ----- 169 D5135 <10 ----- 171 D5135 <1 ----- 173 D5135 6 ----- 174 D5135 <10 ----- 273 ----- ----- 311 D5135 <10 ----- 323 D5135 <10 ----- 333 ----- ----- 343 D5135 <10 ----- 347 D5135 <10 ----- 396 ----- ----- 446 D5135 <10 ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 <10 ----- 858 D5135 <10 ----- 860 D5135 <10 ----- 862 D5135 <10 ----- 863 D5135 <10 ----- 868 D5135 <10 ----- 869 ----- ----- 902 ----- ----- 913 D5135 <5 -----

1067 ----- ----- 1107 D5135 <10 ----- 1117 D5135 7 ----- 1201 D5135 1 ----- 1252 D5135 8.2 ----- 1264 ----- ----- 1319 Less than 4 ----- 1429 ----- ----- 1509 D5135 5 ----- 1515 D7504 5 ----- 1767 ----- ----- 1823 D5135 <10 ----- 1866 ----- ----- 1880 D5135 4.4 ----- 6013 ----- ----- 7014 D5135 1.7 ----- 9008 D5135 <10 -----

normality n.a. n 28 outliers 0 mean (n) <10 st.dev. (n) n.a. R(calc.) n.a. R(D5135:14) n.a.



Determination of iso-Propylbenzene (Cumene) on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 4 ----- 169 D5135 <10 ----- 171 D5135 <1 ----- 173 D5135 4 ----- 174 D5135 <10 ----- 273 ----- ----- 311 D5135 <10 ----- 323 D5135 <10 ----- 333 D5135 <10 ----- 343 D5135 <10 ----- 347 D5135 <10 ----- 396 ----- ----- 446 D5135 <10 ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 <10 ----- 858 D5135 <10 ----- 860 D5135 <10 ----- 862 D5135 3 ----- 863 D5135 <10 ----- 868 D5135 <10 ----- 869 D5135 <10 ----- 902 ----- ----- 913 D5135 nd -----

1067 ----- ----- 1107 D5135 <10 ----- 1117 D5135 3 ----- 1201 D5135 <10 ----- 1252 D5135 4.0 ----- 1264 ----- ----- 1319 5.0 ----- 1429 ----- ----- 1509 D5135 <5 ----- 1515 D7504 <5 ----- 1767 ----- ----- 1823 D5135 2.2 ----- 1866 ----- ----- 1880 D5135 3.3 ----- 6013 ----- ----- 7014 D5135 3.1 ----- 9008 D5135 <10 -----




Determination of o-Xylene on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 2 ----- 169 D5135 33 DG(0.05) ----- possibly a false positive test result? 171 D5135 30 DG(0.05) ----- possibly a false positive test result? 173 D5135 14 ----- 174 D5135 <10 ----- 273 ----- ----- 311 D5135 10 ----- 323 D5135 <10 ----- 333 D5135 15 ----- 343 D5135 <10 ----- 347 D5135 <10 ----- 396 ----- ----- 446 D5135 <10 ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 <10 ----- 858 D5135 <10 ----- 860 D5135 <10 ----- 862 D5135 <10 ----- 863 D5135 <10 ----- 868 D5135 <10 ----- 869 ----- ----- 902 ----- ----- 913 D5135 nd -----

1067 ----- ----- 1107 D5135 <10 ----- 1117 D5135 2 ----- 1201 D5135 <10 ----- 1252 D5135 2.5 ----- 1264 ----- ----- 1319 2.0 ----- 1429 ----- ----- 1509 D5135 <5 ----- 1515 D7504 <5 ----- 1767 ----- ----- 1823 D5135 <10 ----- 1866 ----- ----- 1880 D5135 1.4 ----- 6013 ----- ----- 7014 D5135 1.3 ----- 9008 D5135 <10 -----

normality n.a. n 23 outliers 2 mean (n) <10 st.dev. (n) n.a. R(calc.) n.a. R(D5135:14) n.a.



Determination of n-Propylbenzene on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 67 0.74 169 D5135 62 -0.15 171 D5135 <1 <-11.02 possibly a false negative test result? 173 D5135 64 0.21 174 D5135 <10 <-9.42 possibly a false negative test result? 273 ----- ----- 311 D5135 70 1.28 323 D5135 65 0.39 333 ----- ----- 343 D5135 57 -1.04 347 D5135 66 0.57 396 ----- ----- 446 ----- ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 62 -0.15 858 D5135 60 -0.50 860 D5135 62 -0.15 862 D5135 61 -0.33 863 D5135 61 -0.33 868 D5135 61 -0.33 869 ----- ----- 902 ----- ----- 913 ----- -----

1067 ----- ----- 1107 D5135 37 R(0.01) -4.60 1117 D5135 64 0.21 1201 D5135 56 -1.22 1252 D5135 69.0 1.10 1264 ----- ----- 1319 66.8 0.71 1429 ----- ----- 1509 D5135 82 R(0.01) 3.42 1515 D7504 54 -1.57 1767 ----- ----- 1823 D5135 66.0 0.57 1866 ----- ----- 1880 D5135 65.3 0.44 6013 ----- ----- 7014 D5135 62.9 0.01 9008 D5135 60.2 -0.47

normality OK n 22 outliers 2 spike mean (n) 62.83 50.3 (recovery: < 125%) st.dev. (n) 4.035 R(calc.) 11.30 R(D5135:14) 15.71 compare R(Horwitz) = 15.09 and R(D1535:16) = R(D1535:14)

20

30

40

50

60

70

80

90

1107

1515

1201

343

858

9008

862

863

868

860

169

857

7014

173

1117

323

1880

347

1823

1319

150

1252

311

1509 0

0.02

0.04

0.06

0.08

0.1

0.12

20 40 60 80 100

Kernel Density



Determination of m- & p-Ethyltoluenes on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 8 -0.86 169 ----- ----- 171 D5135 <1 <-6.96 possibly a false negative test result? 173 D5135 10 0.89 174 D5135 <10 ----- 273 ----- ----- 311 D5135 <10 ----- 323 ----- ----- 333 ----- ----- 343 D5135 <10 ----- 347 ----- ----- 396 ----- ----- 446 ----- ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 ----- ----- 858 ----- ----- 860 ----- ----- 862 D5135 8 -0.86 863 D5135 <10 ----- 868 D5135 <10 ----- 869 ----- ----- 902 ----- ----- 913 ----- -----

1067 ----- ----- 1107 ----- ----- 1117 D5135 9 0.02 1201 ----- ----- 1252 D5135 10.2 1.07 1264 ----- ----- 1319 9.6 0.54 1429 ----- ----- 1509 D5135 10 0.89 1515 D7504 5 D(0.05) -3.47 1767 ----- ----- 1823 D5135 8.3 -0.59 1866 ----- ----- 1880 D5135 8.7 -0.24 6013 ----- ----- 7014 D5135 8 -0.86 9008 D5135 <10 -----

normality OK n 10 outliers 1 mean (n) 8.98 st.dev. (n) 0.905 R(calc.) 2.53 R(D5135:14) 3.21 compare R(Horwitz 2 comp) = 4.09 and R(D1535:16) = 4.53

0

2

4

6

8

10

12

14

1515

150

862

7014

1823

1880

1117

1319

173

1509

1252 0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0.45

0.5

0 5 10 15

Kernel Density



Determination of α-Methylstyrene on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 216 -0.97 169 D5135 200 -2.17 171 D5135 205 -1.79 173 D5135 229 0.00 174 D5135 236.8 0.58 273 ----- ----- 311 D5135 200 -2.17 323 D5135 262 2.45 333 D5135 225 -0.30 343 D5135 190 -2.91 347 D5135 212 -1.27 396 ----- ----- 446 D5135 247 1.34 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 236 0.52 858 D5135 250 1.56 860 D5135 247 1.34 862 D5135 249 1.49 863 D5135 246 1.26 868 D5135 237 0.59 869 D5135 248 1.41 902 ----- ----- 913 ----- -----

1067 ----- ----- 1107 D5135 215 -1.05 1117 D5135 204 -1.87 1201 D5135 172 -4.25 1252 D5135 196.8 -2.40 1264 ----- ----- 1319 269 2.98 1429 ----- ----- 1509 D5135 228 -0.08 1515 D7504 226 -0.23 1767 ----- ----- 1823 ----- ----- 1866 ----- ----- 1880 D5135 262.8 2.51 6013 ----- ----- 7014 D5135 252.9 1.78 9008 D5135 251.4 1.66

normality OK n 28 outliers 0 mean (n) 229.06 st.dev. (n) 24.786 R(calc.) 69.40 R(D5135:14) 37.57 compare R(Horwitz) = 45.29 and R(D1535:16) = 38.67

150

170

190

210

230

250

270

290

1201

343

1252

311

169

1117

171

347

1107

150

333

1515

1509

173

857

174

868

863

860

446

869

862

858

9008

7014

323

1880

1319 0

0.002

0.004

0.006

0.008

0.01

0.012

0.014

0.016

0.018

100 150 200 250 300 350

Kernel Density



Determination of 1,2-Diethylbenzene on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 ----- ----- 169 ----- ----- 171 D5135 <1 ----- possibly a false negative test result? 173 ----- ----- 174 D5135 20.5 ----- 273 ----- ----- 311 D5135 50 ----- 323 ----- ----- 333 ----- ----- 343 ----- ----- 347 ----- ----- 396 ----- ----- 446 ----- ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 ----- ----- 858 ----- ----- 860 ----- ----- 862 ----- ----- 863 ----- ----- 868 ----- ----- 869 ----- ----- 902 ----- ----- 913 ----- -----

1067 ----- ----- 1107 ----- ----- 1117 D5135 63 ----- 1201 D5135 58 ----- 1252 ----- ----- 1264 ----- ----- 1319 ----- ----- 1429 ----- ----- 1509 ----- ----- 1515 D7504 <5 ----- possibly a false negative test result? 1767 ----- ----- 1823 ----- ----- 1866 ----- ----- 1880 ----- ----- 6013 ----- ----- 7014 ----- ----- 9008 ----- -----

normality unknown n 4 outliers 0 spike mean (n) 47.88 50.5 (recovery <95%) st.dev. (n) 19.019 R(calc.) 53.25 R(Horwitz) (11.98)



Determination of sum of α-Methylstyrene and 1,2-Diethylbenzene on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 ----- ----- 169 ----- ----- 171 D5135 205 -1.79 173 ----- ----- 174 D5135 257.3 0.34 273 ----- ----- 311 D5135 250 0.05 323 ----- ----- 333 ----- ----- 343 ----- ----- 347 ----- ----- 396 ----- ----- 446 ----- ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 ----- ----- 858 ----- ----- 860 ----- ----- 862 ----- ----- 863 ----- ----- 868 ----- ----- 869 ----- ----- 902 ----- ----- 913 ----- -----

1067 ----- ----- 1107 ----- ----- 1117 D5135 267 0.74 1201 D5135 230 -0.77 1252 ----- ----- 1264 ----- ----- 1319 283.5 1.41 1429 ----- ----- 1509 ----- ----- 1515 D7504 226 -0.93 1767 ----- ----- 1823 D5135 272.1 0.95 1866 ----- ----- 1880 ----- ----- 6013 ----- ----- 7014 ----- ----- 9008 ----- -----

normality unknown n 8 outliers 0 mean (n) 248.86 st.dev. (n) 26.575 R(calc.) 74.41 R(Horwitz 2 comp) 68.73

100

150

200

250

300

350

171

1515

1201

311

174

1117

1823

1319 0

0.002

0.004

0.006

0.008

0.01

0.012

0.014

0.016

100 150 200 250 300 350

Kernel Density



Determination of Phenylacetylene on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 6 ----- 169 D5135 <10 ----- 171 D5135 <1 ----- 173 D5135 5 ----- 174 D5135 <10 ----- 273 ----- ----- 311 D5135 10 ----- 323 D5135 <10 ----- 333 D5135 <10 ----- 343 ----- ----- 347 D5135 <10 ----- 396 ----- ----- 446 D5135 <10 ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 11 ----- 858 D5135 <10 ----- 860 D5135 <10 ----- 862 D5135 <10 ----- 863 D5135 9 ----- 868 ----- ----- 869 D5135 <10 ----- 902 ----- ----- 913 ----- -----

1067 ----- ----- 1107 D5135 5 ----- 1117 D5135 12 ----- 1201 D5135 <10 ----- 1252 D5135 6.3 ----- 1264 ----- ----- 1319 3.4 ----- 1429 ----- ----- 1509 D5135 7 ----- 1515 D7504 <5 ----- 1767 ----- ----- 1823 ----- ----- 1866 ----- ----- 1880 D5135 11.1 ----- 6013 ----- ----- 7014 D5135 9.3 ----- 9008 D5135 <10 -----




Determination of 3- & 4-Methylstyrenes on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 ----- ----- 169 ----- ----- 171 D5135 <1 ----- 173 ----- ----- 174 D5135 22.6 ----- possibly a false positive test result? 273 ----- ----- 311 D5135 <10 ----- 323 ----- ----- 333 ----- ----- 343 ----- ----- 347 ----- ----- 396 ----- ----- 446 ----- ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 ----- ----- 858 ----- ----- 860 ----- ----- 862 ----- ----- 863 ----- ----- 868 ----- ----- 869 ----- ----- 902 ----- ----- 913 ----- -----

1067 ----- ----- 1107 ----- ----- 1117 D5135 <5 ----- 1201 D5135 <10 ----- 1252 ----- ----- 1264 ----- ----- 1319 9.5 ----- 1429 ----- ----- 1509 ----- ----- 1515 D7504 8 ----- 1767 ----- ----- 1823 ----- ----- 1866 ----- ----- 1880 ----- ----- 6013 ----- ----- 7014 ----- ----- 9008 ----- -----




Determination of sum Phenylacetylene and 3-&4-Methylstyrenes on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 ----- ----- 169 ----- ----- 171 D5135 <1 <-4.66 possibly a false negative test result? 173 ----- ----- 174 D5135 22.6 D(0.05) 5.83 273 ----- ----- 311 D5135 10 -0.29 323 ----- ----- 333 ----- ----- 343 ----- ----- 347 ----- ----- 396 ----- ----- 446 ----- ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 ----- ----- 858 ----- ----- 860 ----- ----- 862 ----- ----- 863 ----- ----- 868 ----- ----- 869 ----- ----- 902 ----- ----- 913 ----- -----

1067 ----- ----- 1107 ----- ----- 1117 D5135 12 0.68 1201 D5135 <20 ----- 1252 ----- ----- 1264 ----- ----- 1319 12.8 1.07 1429 ----- ----- 1509 ----- ----- 1515 D7504 8 -1.26 1767 ----- ----- 1823 D5135 10.2 -0.19 1866 ----- ----- 1880 ----- ----- 6013 ----- ----- 7014 ----- ----- 9008 ----- -----

normality unknown n 5 outliers 1 mean (n) 10.60 st.dev. (n) 1.876 R(calc.) 5.25 R(Horwitz 3 comp) 5.77

0

5

10

15

20

25

1515 311

1823

1117

1319 174



Determination of Benzaldehyde on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 74 1.84 169 ----- ----- 171 D5135 70 1.10 173 D5135 70 1.10 174 D5135 <10 <-9.86 possibly a false negative test result? 273 ----- ----- 311 D5135 70 1.10 323 D5135 48 -2.92 333 ----- ----- 343 ----- ----- 347 D5135 49 -2.73 396 ----- ----- 446 ----- ----- 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 D5135 69 0.92 858 D5135 70.2 1.14 860 D5135 67 0.56 862 D5135 66 0.37 863 ----- ----- 868 ----- ----- 869 ----- ----- 902 ----- ----- 913 ----- -----

1067 ----- ----- 1107 ----- ----- 1117 D5135 55 -1.64 1201 D5135 52 -2.18 1252 ----- ----- 1264 ----- ----- 1319 60.0 -0.72 1429 ----- ----- 1509 D5135 68 0.74 1515 ----- ----- 1767 ----- ----- 1823 D5135 71.6 1.40 1866 ----- ----- 1880 ----- ----- 6013 ----- ----- 7014 D5135 63.5 -0.08 9008 ----- -----

normality OK n 16 outliers 0 mean (n) 63.96 st.dev. (n) 8.487 R(calc.) 23.76 R(Horwitz) 15.32 compare R(D5135:16) = 23.98

30

40

50

60

70

80

90

323

347

1201

1117

1319

7014

862

860

1509

857

311

173

171

858

1823

150 0

0.01

0.02

0.03

0.04

0.05

0.06

20 40 60 80 100

Kernel Density



Determination of Nonaromatics on sample #16200; results in mg/kg

lab method value mark z(targ) remarks 150 D5135 76 0.95 169 ----- ----- 171 D5135 73 0.76 173 D5135 104 2.73 174 D5135 20.86 -2.54 273 ----- ----- 311 D5135 40 -1.33 323 D5135 68 0.45 333 ----- ----- 343 ----- ----- 347 D5135 86 1.59 396 ----- ----- 446 D5135 48 -0.82 551 ----- ----- 557 ----- ----- 613 ----- ----- 857 ----- ----- 858 ----- ----- 860 ----- ----- 862 ----- ----- 863 ----- ----- 868 D5135 85 1.52 869 ----- ----- 902 ----- ----- 913 ----- -----

1067 ----- ----- 1107 ----- ----- 1117 D5135 63 0.13 1201 D5135 41 -1.27 1252 D5135 <1 <-3.80 possibly a false negative test result? 1264 ----- ----- 1319 70 0.57 1429 ----- ----- 1509 ----- ----- 1515 D7504 22 -2.47 1767 ----- ----- 1823 D5135 10.4 -3.21 1866 ----- ----- 1880 ----- ----- 6013 ----- ----- 7014 ----- ----- 9008 D5135 107.2 2.93

normality OK n 15 outliers 0 mean (n) 60.96 st.dev. (n) 29.749 R(calc.) 83.30 R(Horwitz 9 comp) 44.14 compare R(D5135:16) = 71.13

0

20

40

60

80

100

120

1823

174

1515

311

1201

446

1117

323

1319

171

150

868

347

173

9008

0

0.002

0.004

0.006

0.008

0.01

0.012

0.014

0.016

-50 0 50 100 150 200

Kernel Density



APPENDIX 2

Number of participants per country

1 lab in AUSTRALIA

2 labs in BELGIUM

2 labs in BRAZIL

1 lab in CANADA

9 labs in CHINA, People's Republic

1 lab in FRANCE

1 lab in INDIA

1 lab in IRAN, Islamic Republic of

1 lab in ITALY

1 lab in JAPAN

2 labs in KUWAIT

4 labs in NETHERLANDS

2 labs in SAUDI ARABIA

1 lab in SINGAPORE

1 lab in SOUTH AFRICA

2 labs in SPAIN

2 labs in TURKEY

1 lab in UNITED ARAB EMIRATES

2 labs in UNITED KINGDOM

5 labs in UNITED STATES OF AMERICA



APPENDIX 3 Abbreviations

C = final test result after checking of first reported suspect test result

D(0.01) = outlier in Dixon’s outlier test

D(0.05) = straggler in Dixon’s outlier test

G(0.01) = outlier in Grubbs’ outlier test

G(0.05) = straggler in Grubbs’ outlier test

DG(0.01) = outlier in Double Grubbs’ outlier test

DG(0.05) = straggler in Double Grubbs’ outlier test

R(0.01) = outlier in Rosner’s outlier test

R(0.05) = straggler in Rosner’s outlier test

W = test result withdrawn on request of participant

ex = test result excluded from calculations

n.a. = not applicable

n.e. = not evaluated

n.d. = not detected

fr. = first reported

SDS = Safety Data Sheet

Literature

1 iis Interlaboratory Studies, Protocol for the Organisation, Statistics & Evaluation, April 2014

2 ASTM E178:02

3 ASTM E1301:03

4 ISO13528:15

5 ISO 5725:86

6 ISO 5725, parts 1-6, 1994

7 M. Thompson and R. Wood, J. AOAC Int, 76, 926, (1993)

8 W.J. Youden and E.H. Steiner, Statistical Manual of the AOAC, (1975)

9 IP 367:84

10 DIN 38402 T41/42

11 P.L. Davies, Fr. Z. Anal. Chem, 331, 513, (1988)

12 J.N. Miller, Analyst, 118, 455, (1993)

13 Analytical Methods Committee Technical brief, No 4 January 2001.

14 P.J. Lothian and M. Thompson, The Royal Society of Chemistry, Analyst, 127, 1359-1364 (2002)

15 Bernard Rosner, Percentage Points for a Generalized ESD Many-Outlier Procedure, Technometrics, 25(2),

165-172, (1983)

16 Horwitz, R. Albert, J. AOAC Int. 79-3, 589 (1996)

results of proficiency test styrene october 2016 - iisnl.com · results of proficiency test styrene...

Documents